Ethanol → HCID 12852073, Verbindung

HRID 1156359Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1156359
[NH2:1][C:2]1[CH:27]=[CH:26][CH:25]=[CH:24][C:3]=1[C:4]([NH:6][CH2:7][CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([C:15](=[O:23])[C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)=[O:5].C=O.[CH2:30](O)C>[OH-].[Na+].O>[F:22][C:19]1[CH:18]=[CH:17][C:16]([C:15]([CH:12]2[CH2:11][CH2:10][N:9]([CH2:8][CH2:7][N:6]3[C:4](=[O:5])[C:3]4[C:2](=[CH:27][CH:26]=[CH:25][CH:24]=4)[NH:1][CH2:30]3)[CH2:14][CH2:13]2)=[O:23])=[CH:21][CH:20]=1

Komponenten

6

Edukt 3

HCID 702EthanolHCID 712FormaldehydeHCID 30186512-Amino-N-{2-[4-(4-fluorobenzoyl)piperidin-1-yl]ethyl}benzene-1-carboximidic acid

Produkt 1

HCID 12852073HCID 12852073, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14798Sodium HydroxideKatalysatorHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 6.5 parts of 2-amino-N-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]benzamide, 0.5 parts of paraformaldehyde, 3 drops of sodium hydroxide solution 50%, 80 parts of ethanol and 10 parts of water is stirred and refluxed overnight. The reaction mixture is allowed to cool to room temperature while stirring. The precipitated product if filtered off, washed with ethanol and crystallized from 200 parts of ethanol, yielding 3.3 parts (50%) of 3-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,3-dihydro-4(1H)-quinazolinone; mp. 203.4° C.

Aufarbeitung

  1. temperaturerefluxed overnight
  2. stirringwhile stirring
  3. filtrationThe precipitated product if filtered off
  4. washwashed with ethanol
  5. customcrystallized from 200 parts of ethanol

Quellen und Nachweise

ORD-Eintrag
ord-ad1ce023a24b4292acc31112460199ea
Quelldatensatz
uspto-grants-1982_06
Patentnummer
US04335127

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